反应详情

105 g (0.39 mols, 1 eq) of 4-nitrobenzoyl-chloroacetic acid ethyl ester are dissolved in 600 ml of THF. To this solution are added, on a water bath (T=35° C.), in portions, 49.4 g (0.37 mols) of finely ground sodium cyanoacetic acid ethyl ester (preparation: Chem, Ber. 1962, 95, 307-318.). It is stirred over night (under N2), fully concentrated by evaporation, and extracted with H2O and CH2Cl2. The combined CH2Cl2 phase is washed with H2O, and finally dried over MgSO4 and freed from solvent. Crystallisation from toluene yields the title compound, m.p.: 174-177° C.

1. additionTo this solution are added, on a water bath (T=35° C.)
2. concentrationfully concentrated by evaporation
3. extractionextracted with H2O and CH2Cl2
4. washThe combined CH2Cl2 phase is washed with H2O
5. dry with materialfinally dried over MgSO4
6. customCrystallisation from toluene